CA2295734A1 - Catalyst component for polymerization of olefins, polymerization catalysts and process of polymerization of olefins by using the same - Google Patents
Catalyst component for polymerization of olefins, polymerization catalysts and process of polymerization of olefins by using the same Download PDFInfo
- Publication number
- CA2295734A1 CA2295734A1 CA002295734A CA2295734A CA2295734A1 CA 2295734 A1 CA2295734 A1 CA 2295734A1 CA 002295734 A CA002295734 A CA 002295734A CA 2295734 A CA2295734 A CA 2295734A CA 2295734 A1 CA2295734 A1 CA 2295734A1
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- Prior art keywords
- polymerization
- olefins
- catalyst component
- radical
- same
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F32/00—Homopolymers and copolymers of cyclic compounds having no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F17/00—Metallocenes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F10/02—Ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F12/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F12/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F12/02—Monomers containing only one unsaturated aliphatic radical
- C08F12/04—Monomers containing only one unsaturated aliphatic radical containing one ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/02—Ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/02—Ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2420/00—Metallocene catalysts
- C08F2420/04—Cp or analog not bridged to a non-Cp X ancillary anionic donor
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/64—Titanium, zirconium, hafnium or compounds thereof
- C08F4/659—Component covered by group C08F4/64 containing a transition metal-carbon bond
- C08F4/65908—Component covered by group C08F4/64 containing a transition metal-carbon bond in combination with an ionising compound other than alumoxane, e.g. (C6F5)4B-X+
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/64—Titanium, zirconium, hafnium or compounds thereof
- C08F4/659—Component covered by group C08F4/64 containing a transition metal-carbon bond
- C08F4/65912—Component covered by group C08F4/64 containing a transition metal-carbon bond in combination with an organoaluminium compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/64—Titanium, zirconium, hafnium or compounds thereof
- C08F4/659—Component covered by group C08F4/64 containing a transition metal-carbon bond
- C08F4/6592—Component covered by group C08F4/64 containing a transition metal-carbon bond containing at least one cyclopentadienyl ring, condensed or not, e.g. an indenyl or a fluorenyl ring
- C08F4/65922—Component covered by group C08F4/64 containing a transition metal-carbon bond containing at least one cyclopentadienyl ring, condensed or not, e.g. an indenyl or a fluorenyl ring containing at least two cyclopentadienyl rings, fused or not
- C08F4/65927—Component covered by group C08F4/64 containing a transition metal-carbon bond containing at least one cyclopentadienyl ring, condensed or not, e.g. an indenyl or a fluorenyl ring containing at least two cyclopentadienyl rings, fused or not two cyclopentadienyl rings being mutually bridged
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S526/00—Synthetic resins or natural rubbers -- part of the class 520 series
- Y10S526/943—Polymerization with metallocene catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
Abstract
The present invention relates to a metallocene compound as a catalyst component for the polymerization of olefins, said compound, is stable to air and moisture so that generates no hydrogen halide by hydrolysis and easily handled, and has a high storage stability arid a high catalyst activity. Specifically, the catalyst component for the polymerization of olefins comprises a transition metal composition represented by the general formula [1] and [2]:
(R a Cp)a (R'b Cp) M (-X-Ar-Y c)4 -(m+n) . . . . [1]
R" (R d Cp) (R'a Cp) M (-X-Ar-Y c)2 . . . . [2]
.wherein M is Ti, Zr or Hf; (R a Cp), (R'b Cp), (R d Cp) and (R"c Cp) each is a radical having the cyclopentadienyl skeleton; R" is a radical which links (R d Cp) and (R'c Cp); (-X-Ar-Y c) is a grouping in which the aromatic ring Ar substituted by a specified radical Y bonds to M through an oxygen or sulphur atom X.
(R a Cp)a (R'b Cp) M (-X-Ar-Y c)4 -(m+n) . . . . [1]
R" (R d Cp) (R'a Cp) M (-X-Ar-Y c)2 . . . . [2]
.wherein M is Ti, Zr or Hf; (R a Cp), (R'b Cp), (R d Cp) and (R"c Cp) each is a radical having the cyclopentadienyl skeleton; R" is a radical which links (R d Cp) and (R'c Cp); (-X-Ar-Y c) is a grouping in which the aromatic ring Ar substituted by a specified radical Y bonds to M through an oxygen or sulphur atom X.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP18419997 | 1997-07-09 | ||
JP9/184199 | 1997-07-09 | ||
PCT/JP1997/004441 WO1999002571A1 (en) | 1997-07-09 | 1997-12-04 | Catalytic components for the polymerization of olefins, polymerization catalysts, and process for polymerizing olefins by using the same |
Publications (2)
Publication Number | Publication Date |
---|---|
CA2295734A1 true CA2295734A1 (en) | 1999-01-21 |
CA2295734C CA2295734C (en) | 2005-02-08 |
Family
ID=16149099
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA002295734A Expired - Fee Related CA2295734C (en) | 1997-07-09 | 1997-12-04 | Catalyst component for polymerization of olefins, polymerization catalysts and process of polymerization of olefins by using the same |
Country Status (8)
Country | Link |
---|---|
US (3) | US6350831B1 (en) |
EP (2) | EP1426386B1 (en) |
JP (1) | JP3244124B2 (en) |
CN (1) | CN100460422C (en) |
CA (1) | CA2295734C (en) |
DE (2) | DE69737368T2 (en) |
TW (1) | TW464658B (en) |
WO (1) | WO1999002571A1 (en) |
Families Citing this family (26)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU2000262096A1 (en) * | 2000-07-12 | 2002-01-21 | E.I. Du Pont De Nemours And Company | Metallocene polymerization catalyst |
JP2002069248A (en) * | 2000-08-30 | 2002-03-08 | Sumitomo Chem Co Ltd | Polyolefin resin composition and film made of the same |
US7923437B2 (en) | 2001-02-16 | 2011-04-12 | Cargill, Incorporated | Water soluble β-glucan, glucosamine, and N-acetylglucosamine compositions and methods for making the same |
US8222232B2 (en) | 2001-02-16 | 2012-07-17 | Cargill, Incorporated | Glucosamine and N-acetylglucosamine compositions and methods of making the same fungal biomass |
US7816514B2 (en) | 2001-02-16 | 2010-10-19 | Cargill, Incorporated | Glucosamine and method of making glucosamine from microbial biomass |
JP2002249527A (en) * | 2001-02-27 | 2002-09-06 | Nippon Zeon Co Ltd | Addition copolymer, hydrogenated addition copolymer, and their production methods |
JP2003012682A (en) * | 2001-06-27 | 2003-01-15 | Sumitomo Chem Co Ltd | Zirconium compound, method for producing the same and use thereof |
US7094723B2 (en) * | 2002-04-18 | 2006-08-22 | Equistar Chemicals Lp | Catalysts containing at least one heterocyclic ligand for improving the catalysts' performance of olefin polymerization |
CN1302016C (en) * | 2002-08-29 | 2007-02-28 | Lg化学株式会社 | Fulvene, metallocene catalysts and preparation method thereof, and preparation of polyolefines copolymer using the same |
DE10250062A1 (en) | 2002-10-25 | 2004-05-06 | Basell Polyolefine Gmbh | New racemic metallocene complexes are useful as catalysts or catalyst components for the polymerization of olefinically unsaturated compounds or as reagents or catalysts in stereoselective syntheses |
US6710005B1 (en) * | 2003-04-10 | 2004-03-23 | Equistar Chemicals, Lp | Aluminoxane modification |
US6930156B2 (en) * | 2003-10-22 | 2005-08-16 | Equistar Chemicals, Lp | Polymer bound single-site catalysts |
JP4133772B2 (en) | 2003-12-01 | 2008-08-13 | 丸善石油化学株式会社 | Olefin polymerization catalyst and olefin polymerization method using the same |
US6967184B2 (en) * | 2004-02-17 | 2005-11-22 | Univation Technologies, Llc | Fluoroalcohol leaving group for non-metallocene olefin polymerization catalysts |
US7125939B2 (en) * | 2004-08-30 | 2006-10-24 | Equistar Chemicals, Lp | Olefin polymerization with polymer bound single-site catalysts |
CN1310970C (en) * | 2005-06-17 | 2007-04-18 | 中国科学院长春应用化学研究所 | Polymerisation catalyst precursor of olefins N and preparation thereof |
US7423098B2 (en) * | 2006-01-17 | 2008-09-09 | Equistar Chemicals, Lp | Polyethylene process |
KR101060838B1 (en) * | 2006-04-24 | 2011-08-30 | 에스케이이노베이션 주식회사 | Bis-arylaryloxy catalyst system for preparing ethylene homopolymer or copolymer with α-olefin |
WO2008008112A1 (en) * | 2006-07-14 | 2008-01-17 | Exxonmobil Chemical Patents Inc. | Ethylene/dicyclopentadiene copolymers and functionalized derivatives thereof |
WO2008060512A1 (en) | 2006-11-14 | 2008-05-22 | Univation Technologies, Llc. | Catalyst systems and polymerization processes |
DE102007009862A1 (en) * | 2007-02-28 | 2008-09-04 | Chemtura Organometallics Gmbh | Preparing bridged, stereo-rigid diphenoxide metallocene compound, useful as a catalyst to prepare polyolefin, comprises reacting a metallocene dihalide compound with an alkylating reagent and reacting the mixture with e.g. phenol |
FR2916199B1 (en) * | 2007-05-14 | 2012-10-19 | Inst Francais Du Petrole | OLEFIN OLIGOMERIZATION METHOD USING A CATALYTIC COMPOSITION COMPRISING AN ORGANOMETALLIC COMPLEX CONTAINING A HETERO-ATOMIC FUNCTIONALIZED PHENOXY LIGAND |
KR101151606B1 (en) * | 2007-12-31 | 2012-06-08 | 에스케이이노베이션 주식회사 | Transition metal complexes, catalysts composition containing the same, and process for preparing ethylene homopolymers or copolymers of ethylene and a-olefins using the same |
US7884165B2 (en) | 2008-07-14 | 2011-02-08 | Chevron Phillips Chemical Company Lp | Half-metallocene catalyst compositions and their polymer products |
KR101077071B1 (en) * | 2008-11-03 | 2011-10-26 | 에스케이이노베이션 주식회사 | Ethylene Copolymer with Improved Impact Resistance |
US9181371B2 (en) | 2011-11-08 | 2015-11-10 | Univation Technologies, Llc | Methods for producing polyolefins with catalyst systems |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3127133A1 (en) | 1981-07-09 | 1983-01-27 | Hoechst Ag, 6000 Frankfurt | METHOD FOR PRODUCING POLYOLEFINS AND THEIR COPOLYMERISATS |
ZA844157B (en) | 1983-06-06 | 1986-01-29 | Exxon Research Engineering Co | Process and catalyst for polyolefin density and molecular weight control |
US4752597A (en) | 1985-12-12 | 1988-06-21 | Exxon Chemical Patents Inc. | New polymerization catalyst |
JPH0780930B2 (en) | 1985-12-26 | 1995-08-30 | 三井石油化学工業株式会社 | Method for polymerizing α-olefin |
US5700750A (en) * | 1985-12-26 | 1997-12-23 | Mitsui Petrochemical Industries, Ltd. | Process for polymerization of alpha-olefins |
DE3800760A1 (en) * | 1988-01-13 | 1989-07-27 | Koepf Maier Petra | CYTOSTATICALLY EFFECTIVE TITANOCEN DERIVATIVES AND MEDICINAL PRODUCTS CONTAINING THEM |
IT1237398B (en) | 1989-01-31 | 1993-06-01 | Ausimont Srl | CATALYSTS FOR THE POLYMERIZATION OF OLEFINE. |
JPH02302410A (en) * | 1989-05-17 | 1990-12-14 | Asahi Chem Ind Co Ltd | Production of highly stereoregular polypropylene |
US5387567A (en) | 1991-06-27 | 1995-02-07 | Nippon Oil Co., Ltd. | Catalyst components for polymerization of olefins |
TW369547B (en) | 1994-09-21 | 1999-09-11 | Mitsui Chemicals Inc | Olefin polymerization catalyst and process for olefin polymerization |
DE69624398T2 (en) * | 1995-03-29 | 2003-06-12 | Univation Tech Llc | Narrow polydispersity ethylene polymers and process for their manufacture |
CN1062275C (en) * | 1995-12-15 | 2001-02-21 | 化学工业部北京化工研究院 | Metallocene catalyst for ethylene polymerization and relevant polymerization method |
US5780659A (en) | 1996-03-29 | 1998-07-14 | Phillips Petroleum Company | Substituted indenyl unbridged metallocenes |
-
1997
- 1997-12-04 JP JP53749298A patent/JP3244124B2/en not_active Expired - Fee Related
- 1997-12-04 WO PCT/JP1997/004441 patent/WO1999002571A1/en active IP Right Grant
- 1997-12-04 CN CNB971822808A patent/CN100460422C/en not_active Expired - Fee Related
- 1997-12-04 DE DE69737368T patent/DE69737368T2/en not_active Expired - Fee Related
- 1997-12-04 EP EP04001780A patent/EP1426386B1/en not_active Expired - Lifetime
- 1997-12-04 EP EP97946101A patent/EP0997480B1/en not_active Expired - Lifetime
- 1997-12-04 DE DE69737776T patent/DE69737776T2/en not_active Expired - Fee Related
- 1997-12-04 CA CA002295734A patent/CA2295734C/en not_active Expired - Fee Related
- 1997-12-10 TW TW086118619A patent/TW464658B/en not_active IP Right Cessation
-
1998
- 1998-12-28 US US09/220,589 patent/US6350831B1/en not_active Expired - Fee Related
-
2000
- 2000-05-16 US US09/571,863 patent/US6323149B1/en not_active Expired - Fee Related
-
2001
- 2001-09-28 US US09/964,432 patent/US6569800B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
EP1426386A1 (en) | 2004-06-09 |
DE69737776D1 (en) | 2007-07-12 |
CN1259963A (en) | 2000-07-12 |
EP1426386B1 (en) | 2007-05-30 |
WO1999002571A1 (en) | 1999-01-21 |
TW464658B (en) | 2001-11-21 |
DE69737776T2 (en) | 2008-01-31 |
JP3244124B2 (en) | 2002-01-07 |
US6323149B1 (en) | 2001-11-27 |
EP0997480B1 (en) | 2007-02-14 |
CA2295734C (en) | 2005-02-08 |
US20020039963A1 (en) | 2002-04-04 |
EP0997480A1 (en) | 2000-05-03 |
CN100460422C (en) | 2009-02-11 |
DE69737368D1 (en) | 2007-03-29 |
DE69737368T2 (en) | 2007-10-31 |
US6350831B1 (en) | 2002-02-26 |
US6569800B2 (en) | 2003-05-27 |
EP0997480A4 (en) | 2000-09-06 |
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